Basic sulfate of zirconium and method of making the same.



EUTKTARD J. PUGH, 039

inn STATE ENT onrion GLENSIDE, PENNSYLVANIA, ASSIGNOR T0 PENNSYLVANIA SALT MANUFACTURING COMPAITY, OF PHILADELlPHIA, PENNSYLVANIA, A CORPORATIUN O]? EENN'SYLVANIA.

BASIC SULFATE GE ZIRCONI'UM AND METHOD OF MAKING THE SAME.

aerator.

l lo Drawing.

To all whom it may concern:

Be it known that l, EDWARD J. Peon, residing at Glenside, Montgomery county, Pennsylvania, have invented new and useful Basic Sulfate of Zirconiumand Methods. of Makin the Same, of which the following is a ll, clear, and exact description.

My invention provides a simple and comparatively inexpensive method, by means of which a substantially pure zirconium oxid may be obtained.

' It has heretofore been roposed to produce zirconium oxid by rst preparing a zirconium oxychlorid and treating this with a definite amount of sulfuric acid, the mixture being allowed to stand in the cold or at about 40 0., when a basic s ulfate of zirconium having the compos tion (SZrUfil-LSOQ separates in small prlsms which are free from iron and titanium. This basic sulfate of zirconium can be converted to zirconium oxid by any well'known method. The method is, however, objectionable in that the time required for the precipitation' of the basic sulfate of zirconlum extends over a great number of days. 'Further, the precipitation is never complete,

less than 75% precipitating out in two weeks.

It has also been proposed to produce zirconium oxid by preparing a sulfate of zirconium, dissolving this in water and adding hydrochloric acid and ammonia, whereby a precipitate of basic sulfate of zirconium having .a composition of (60-66%, zro,, 10 15%so,-) is obtained. I a a lit has also been proposed to use an oxychlorid of zirconium of a composition Zr,O,Cl,22H,O, which is dissolved in water and a definite quantity of sulfuric acid added, whereby basic sulfate is precipitated having the composition 5ZrO 2SO,14H,O.

The first named of these twomethods is expensive on account of the use of'ammonia which is required, and the product obtained is an impure one, which must be purified by later processes where a pure product is desired. The last-named method is expensive, since a weak solution containing hydrochloric acid must be evaporated and since only a part of the zirconium is converted into the desired new basic oxychlorid.

Specification of Letters Patent. Patented Sept. 16, 1919. Application filed July 15, 1am. Serial No. 245,046. I

I have discovered. that a new basic sulfate of zirconium substantially free from iron, titanium and silicon and which may be converted to pure zirconium oxid by wellknown methods, may be simply and cheaply produced as follows: Oxychlorid of zir conium which has been manufactured by any of the well-known methods is dissolved insufficient water to form a solution con- "and capable of ready conversion to pure zirconium oxid in an wellknown manner.

As a more speci c example, a quantity-of zirconium oxychlorid containing 100 grams of zirconium oxid is dissolved in three liters of water; this solution is acidified with hydrochloric acid and an addition of 48 grams of sulfuric acid is made. Upon heating, the

precipitate above described is obtained.

I do notdesire to limit myself to the particular proportipns and temperatures which I have herein'given, as these may be varied within the spirit and scppe ofthe appended claims.

I claim: a 1. As a new artlcle of manufacture, a

basic sulfate of zirconium, consisting of the precipitate resulting from the addition of sulfuric acid to an acid solution of zirconium oxychlorid in the proportion of 5Zr0 to 311 30,.

a 2. As a new article of. manufacture, a

" basic sulfate of zirconium, consisting of the precipitate resulting from the addltion of sulfurlc acid to a solution of zirconium oxy- Chlgl'ld, 1n the presence of hydrochloric ac1 i As a new article of manufacture, a zirconium basic sulfate having substantially the composition 5Zr0 3SO 13H,O.

4:. The herein described method of mak- I ing a new basic sulfate of zirconium which consists in adding sulfuric acid to an acid solution of zirconium oxychlorid and heating the same. Y

5. The herein described method of making a basic sulfate of zirconium which consists in adding sulfuric acid to a solution of zirconlum oxychlorld 1n the presence of hydrochlorlc acid and heating the same.

In testimon my hand.

y whereof I have hereunto set 10 EDWARD J. PUGH. 

